Manufacture of rayon



United States Patent Ofifice 3,026,171 Patented Mar. 20, 1962 3,026,171MANUFACTURE OF RAYON Nikolaus Augustin Schonfeldt, Molndal, and KurtHelmut Grunewald, Goteborg, Sweden, assignors, by mesne assignments, toAmerican Enka Corporation, Enka, N.C., a corporation of Delaware NoDrawing. Original application Mar. 23, 1953, Ser. No. 344,182. Dividedand this application Sept. 28, 1959, Ser. No. 842,575

Claims. (Cl. 18-54) This application is a division of our copendingapplication Serial No. 344,182, filed March 23, 1953, and now abandoned.

The present invention relates to the manufacture of viscose rayon yarns,films and the like, and more particularly to the production of rayon inthe presence of a quaternary ammonium compound.

In recent years, it has been determined that improved rayon yarns, filmsand the like could be manufactured by the use of modifiers that retardthe regeneration processes in the viscose and thereby permit higherstretches which improved both the strength and fatigue. Some of thesemodifiers have been described in US. Patent Nos. 2,535,044, 2,535,045,and 2,536,014.

It is therefore an object of the present invention to provide a processfor the manufacture of rayon yarns, films, and the like of improvedstrength and fatigue.

Another object of this invention is to provide a process for themanufacture of rayon in which the filaments have improvedstretchability.

An additional object of this invention is to provide a process for themanufacture of rayon wherein spinneret incrustation is inhibited.

A further object of this invention is to provide a process for themanufacture of rayon wherein the filterability of the viscose isimproved.

A still further object of this invention is to provide a process for theproduction of viscose of improved clarity.

It is an additional object of this invention to provide an improvedviscose spinning solution.

These and other objects are accomplished by incorporating into theviscose at some stage in the processing a surface active, quaternaryammonium compound of the general formula:

wherein R is an aliphatic radical containing at least 8 carbon atoms, Ris a radical selected from the group consisting of oxyalkylene orpolyoxyalkylene radicals, R" is an alkyl radical having not more than 2carbon atoms, and X is an innocuous anion consisting of or containing,e.g., a halogen, a 80 1-1 group and a SO CH group.

These compounds may be prepared by quaternizing a compound of thefollowing formula:

/R'H RN wherein R is an aliphatic radical containing at least 8 carbonatoms and R is a radical selected from the group consisting ofoxyalkylene and polyoxyalkylene radicals. In the preferred compounds, Rshould be an aliphatic radical having 8 to 20 carbon atoms such asoctyl, dodecyl, hexadecyl, and octadecyl.

The compound preferably contains 3 to 30 oxyalkylene radicals, out itmay contain more or less. The oxyalkylene radical normally will beethylene oxide, but it may also be propylene oxide or substitutedethylene oxides.

The quaternization of these compounds may be, as for example, bycondensation with alkyl halides such as ethyl chloride, or by reactionwith an alkyl sulfate such as dimethyl sulfate or diethyl sulfate.

These quaternary ammonium compounds may be added at any stage of theprocess of manufacturing regenerated cellulose yarns. Thus it ispossible to obtain improvements in this process by adding thesecompounds to the dissolving liquor, to the viscose solution, to thecarbon disulfide during xanthation, to the steeping liquor, to thealkali cellulose spinning solution, or to the coagulating spinbath.

It is possible by the use of these compounds to improve thefilterability and clarity of the viscose. It is also possible toincrease the amount of stretch to which the filaments may be subjectedduring coagulation. In addition, they permit the production of a moreuniform fiber.

Such quaternary ammonium compounds also inhibit the formation ofspinneret incrustations as well as the inhibition of the formation ofcraters on the spinneret. In addition, it has been found that thesecompounds do not foam, thereby making them particularly adaptable in theprocess.

These results are obtained by choosing the proper compound for thedesired improvements. Thus the selection of the various radicalsmentioned above, as well as the point in the processing at which thematerial is used, depends upon the desired improvements. Each compoundis not necessarily limited to improving one characteristic of theprocess but may improve several. For example, one that improves viscosefilterability may also inhibit spinneret incrustations.

Such compounds, depending upon their composition, may be soluble ordispersible in 18-20% sodium hydroxide and others may be soluble ordispersible in the spinning bath. These properties depend upon thecompounds used in their manufacture as well as the method of production.These compounds may be liquids or solids, which also depends upon theircomposition.

In some cases, it may be desirable to use these compounds in conjunctionwith other agents. Thus if they are used for emulsification, it may bedesirable to use an emulsifying agent in combination with the quaternaryammonium compound.

These compounds may be added to the process in varying amounts,depending upon the desired result. Thus, it is possible to use an amountvarying from 0.045% to 0.09%, based on the Weight of the viscose. Othersamounts may also be used.

The following examples will illustrate the various improvements obtainedby the use of these quaternary ammonium compounds. These examples areincluded merely for the purpose of illustration and are not intended aslimiting the scope of this invention.

Example I Lauryl amine was condensed with 4 moles of ethylene oxide andthe condensation product was reacted with dimeth-yl sulfate to obtain aquaternary ammonium compound of the formula:

(HELD-01114011 SO4CHa" CEHO C2H4OH A dispersion of this product wasprepared in 20% sodium hydroxide so that the dispersion contained 0.2 g.of

this product. This compound increased the reactivity of the alkalicellulose.

Example II Stearyl amine was condensed with 20 moles of ethylene oxideand the condensation product was reacted with dimethyl sulfate to obtaina compound of the formula:

wherein y+z equals 20. This product in an amount of 0.5 g. per liter ofviscose (about 0.045% based on the weight of the viscose) improves theclarity of the viscose and at the same time inhibits clogging of thespinnerets in the spinbath.

Example 111 Hexadecyl amine was condensed with 10 moles of propyleneoxide and the resulting condensation product was reacted with dimethylsulfate to obtain the quaternary ammonium compound of the formula:

CH3 (C3I O) 11 o in -N 804C113- s sO) 2H wherein y-l-z equals 10. Onepart of this compound per 1000 parts of CS was added to the CS with aresulting improvement in emulsion xanthation.

Example IV Lauryl amine was condensed with 5 moles of ethylene oxide andthe condensation product was reacted with dimethyl sulfate to obtain acompound of the formula:

wherein y+z equals 5. One gram of this compound per liter of thecoagulating spinbath inhibited the formation of spinneret craters.

The foregoing examples illustrate that the quaternary ammonium compoundsof this invention may be used in various ways to improve the processingof viscose yarn as Well as improving the yarn itself.

The foregoing description is intended for the purpose of illustration,it being understood that departures from and modifications of thisdescription may be made without departing from the spirit and scope ofthis invention which is to be limited only by the following claims.

The foregoing examples illustrate that the quaternary ammonium compoundsof this invention may be used in various ways to improve the processingof viscose yarn as well as improving the yarn itself.

The foregoing description is intended for the purpose of illustration,it being understood that departures from and modifications of thisdescription may be made without departing from the spirit and scope ofthis invention which is to be limited only by the following claims.

What is claimed is:

1. In the manufacture of viscose yarn wherein a viscose solution isextruded through minute orifices into a coagulating spinbath to formfilaments therefrom, the step which comprises spinning the viscosefilaments in the presence of at least 0.045%, based on the weight of theviscose, of a quaternary ammonium compound represented by the followingformula:

RO) H wherein R is an aliphatic hydrocarbon radical containing at least8 carbon atoms, R is an alkylene radical having from 2 to 3 carbonatoms, R" is an alkyl radical having from one to two carbon atoms, X isa halogen, and x and y are integers having a sum total varying between 3and 30.

2. In the manufacture of viscose yarn according to claim 1, wherein R isan aliphatic radical containing 12-20 carbon atoms. a

3. In the manufacture of viscose yarn according to claim 1, wherein R isa methyl group.

4. In the manufacture of viscose yarn according to claim 1, wherein R isan alkylene radical having 2 carbon atoms.

5. In the manufacture of viscose yarn wherein a viscose solution isextruded through minute orifices into a coagulating spinbath to formfilaments therefrom, the step which comprises spinning the viscosefilaments in the presence of a suflicient amount of a quaternaryammonium compound to modify the properties of the yarn, said compoundbeing represented by the following formula:

wherein R is an aliphatic hydrocarbon radical containing at least 8carbon atoms, R is an alkylene radical having from 2 to 3 carbon atoms,R" is an alkyl radical having from one to two carbon atoms, X is ananion selected from the group consisting of a halogen, an SO H group,and an SO CH group, and x and y are integers having a sum total varyingbetween 3 and 30.

References Cited in the file of this patent UNITED STATES PATENTS2,759,975 Chiddix et al Aug. 21, 1956 Disclaimer 3,026,171.Nik0lausAugustin Schonfeldt, Molndal, and Kurt H ehnut G'mmewald, Goteborg,Sweden. MANUFACTURE or RAYON. Patent dated Mar. 20, 1962. Disclaimerfiled Apr. 9, 1962, by the assignee, American E nka Oorpomtio'n. Herebydisclaims the residual term of said Letters Patent from Mar. 7,

1978 until Mar. 20,1979.

[Oflicz'al Gazette M ay $82, 1962.]

5. IN THE MANUFACTURE OF VISCOSE YARN WHEREIN A VISCOSE SOLUTION ISEXTRUDED THROUGH MINUTE ORIFICES INTO A COAGULATING SPINBATH TO FORMFILAMENTS THEREFROM, THE STEP WHICH COMPRISES SPINNING THE VISCOSEFILAMENTS IN THE PRESENCE OF A SUFFICIENT AMOUNT OF A QUATERNARYAMMONIUM COMPOUND TO MODIFY THE PROPERTIES OF THE YARN, SAID COMPOUNDBEING REPRESENTED BY THE FOLLOWING FORMULA: